CN109019534A - A kind of preparation method of ultrathin boron nitride nanosheet - Google Patents
A kind of preparation method of ultrathin boron nitride nanosheet Download PDFInfo
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- CN109019534A CN109019534A CN201811146892.0A CN201811146892A CN109019534A CN 109019534 A CN109019534 A CN 109019534A CN 201811146892 A CN201811146892 A CN 201811146892A CN 109019534 A CN109019534 A CN 109019534A
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- boron nitride
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- nitride nanosheet
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- ultrathin boron
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 53
- 239000002135 nanosheet Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 230000001681 protective effect Effects 0.000 claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004327 boric acid Substances 0.000 claims abstract description 8
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 10
- 238000003786 synthesis reaction Methods 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- TZHYBRCGYCPGBQ-UHFFFAOYSA-N [B].[N] Chemical compound [B].[N] TZHYBRCGYCPGBQ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 18
- 238000010586 diagram Methods 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 238000006555 catalytic reaction Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention provides a kind of preparation method of ultrathin boron nitride nanosheet, comprising the following steps: (1) is put into tube furnace after mixing boric acid and urea with the ratio of 1:1~1:50；(2) 500~1000 DEG C are heated to 1~15 DEG C/min heating rate under protective atmosphere, cooled to room temperature obtains ultrathin boron nitride nanosheet after keeping the temperature 2~15h.The present invention utilizes the ultrathin boron nitride nanosheet of boron nitrogen precursor synthesis cheap and easy to get, has apparent visible light-responded and preferable photocatalytic activity, and synthetic method is simple, it is easy to accomplish large-scale production.
Description
Technical field
The present invention relates to catalysis material technical fields, more particularly to one kind is for light-catalysed active ultrathin boron nitride nanometer
The preparation method of piece.
Background technique
In recent years, ultra-thin two-dimensional material is widely paid close attention to due to its excellent physicochemical properties.Super thin hexagonal
Phase boron nitride has the characteristics that porous as bi-dimensional cellular shape catalysis material.Simultaneously compared to carbon-based material, such as graphene,
Hexagonal phase boron nitride material not only has excellent thermal stability, will not decompose for 1200 DEG C in air, under vacuum conditions
1600 DEG C will not decompose, at the same it have good chemical stability, can strong alkali-acid resistance corrosion.Therefore, hexagonal phase boron nitride
Material receives the concern and research of more and more people in catalytic field.But hexagonal phase boron nitride forbidden bandwidth is 5.9eV, only right
Ultraviolet light has response, limits it in the further development of photocatalysis field.Currently, there are no correlations to report in photocatalysis field
Hexagonal phase boron nitride is used for gas phase catalysis CO by road2Conversion and go the research of denitrification.
In the means of the passing ultra-thin hexagonal phase boron nitride material of synthesis, common method has chemical vapour deposition technique
(Nano Lett., 2010,10,3209.), mechanical layer stripping (J.Mater.Chem., 2011,21,11862.), ultrasonic wave added
Solution layer stripping (Appl.Phys.Lett., 2008,93,223103.) etc..Above method synthesis technology is complicated, to equipment requirement
Higher, low yield is unfavorable for the ultra-thin hexagonal phase boron nitride material of large scale preparation.And high-temperature sintering process technique is relatively easy, leads to
The ultra-thin hexagonal phase boron nitride nanosheet of different-thickness can be obtained in the ratio for crossing control boron nitrogen presoma.But in existing side
In method, the synthesis temperature of ultra-thin hexagonal phase boron nitride material is prepared mostly more than 1200 DEG C, carrier gas is usually inflammable ammonia, preceding
The preparation process for driving body is complex, the material prepared need subsequent could to use after secondary cleaning (Sci.Rep., 2013,
3,1.ACS Appl.Mater.Interfaces,2017,9,14506.ACS nano,2010,4,1539.ACS Nano
2013,7,1558.).These limitations, so that high-temperature sintering process can not be applied in actual production.Therefore, a kind of technique is invented
Simply, economic security, the preparation method with visible light-responded ultra-thin hexagonal phase boron nitride nanosheet that can be prepared on a large scale
It is extremely urgent.
Summary of the invention
It is an object of the invention to solve the problems of the above-mentioned prior art, a kind of use of simple mild condition is provided
In the preparation method of light-catalysed active ultrathin boron nitride nanosheet, comprising the following steps:
(1) boric acid and urea obtained mixture is mixed in certain proportion to be put into tube furnace；
(2) 500~1000 DEG C are risen to 1~15 DEG C/min of rate under protective atmosphere, keeps the temperature natural cooling after 2~15h
Ultrathin boron nitride nanosheet is obtained to room temperature.
Further, the preparation method of catalysis material as described above, in step (1), a kind of catalysis material of oxygen
The preparation method of material, comprising the following steps:
(1) boric acid and urea obtained mixture is mixed in certain proportion to be put into tube furnace；
(2) 500~1000 DEG C are risen to 1~15 DEG C/min of rate under protective atmosphere, keeps the temperature natural cooling after 2~15h
Ultrathin boron nitride nanosheet is obtained to room temperature.
Further, the preparation method of catalysis material as described above, in step (1), the mixture includes
Boric acid and urea mass ratio be 1:1~1:50.
Further, the preparation method of catalysis material as described above, in step (2), the protective atmosphere
For nitrogen or argon gas.
Further, the preparation method of catalysis material as described above, in step (2), the protective atmosphere is nitrogen
When gas or argon gas, gas flow rate be 30~1200 milliliters/per minute.
The present invention has been synthesized by high temperature method applied to the ultra-thin with visible of photocatalysis field using urea and boric acid
The active hexagonal phase boron nitride nanometer sheet material of photoresponse, it is not simple only with respect to operated in accordance with conventional methods, it is low in cost, be conducive to
Large-scale commercial application, simultaneously synthesizing material have accordingly visible light, and thickness removes field in 1~4nm, in nitrogen oxides
There is certain application prospect.
Detailed description of the invention
Fig. 1 is the XRD diagram of the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention；
Fig. 2 is TEM (a) and HRTEM (b) electron microscope of the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention；
Fig. 3 is the AFM figure of the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention；
Fig. 4 is the UV-Vis DRS abosrption spectrogram (a) of the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention
With partial enlarged view (b)；
Fig. 5 is that the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention is degraded NO efficiency schematic diagram (a) under full spectrum
With generation NO2 production quantity real-time monitoring schematic diagram (b)；
Fig. 6 is that the ultrathin boron nitride nanosheet of present example preparation carries out CO under full spectrum2+H2The CO that O reacts
(a)、H2(b) and CH4(c) yield schematic diagram；
Fig. 7 is that the ultrathin boron nitride nanosheet of present example preparation is dispersed in water the schematic diagram to form colloid.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear
Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment:
Boric acid and urea obtained mixture is mixed with the ratio of 1:1~1:50 first to be put into tube furnace；
Later, 500~1000 DEG C are risen to 1~15 DEG C/min of rate under protective atmosphere (nitrogen or argon gas), heat preservation 2~
Cooled to room temperature obtains ultrathin boron nitride nanosheet after 15h.
Fig. 1 is the XRD diagram of ultrathin boron nitride nanosheet manufactured in the present embodiment, in figure at 26 ° and 43 ° two of appearance it is bright
The aobvious diffraction maximum for belonging to hexagonal phase boron nitride (002) and (100) feature crystal face, it was demonstrated that the material of synthesis is hexagonal phase nitridation
Boron.
Fig. 2 is TEM (a) and HRTEM (b) electron microscope of the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention, from figure
In it can be seen that synthesis hexagonal phase boron nitride nanosheet than relatively thin, thickness is in 1~3nm.
Fig. 3 is the AFM figure of the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention, six as can be seen from the figure synthesized
Square phase boron nitride nanometer sheet with a thickness of 2~4nm.
Fig. 4 is the UV-Vis DRS abosrption spectrogram (a) of the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention
With partial enlarged view (b), the hexagonal phase boron nitride nanosheet as can be seen from the figure synthesized visible light region (420~
700nm) there is certain absorption.
Fig. 5 is that the ultrathin boron nitride nanosheet of preparation of the embodiment of the present invention is degraded NO efficiency schematic diagram (a) under full spectrum
With generation NO2Production quantity real-time monitoring schematic diagram (b) as can be seen from the figure compares the boron nitride of business, the hexagonal phase of synthesis
Boron nitride nanosheet has certain NO degradation capability, while NO2Production quantity is considerably less, less than 1%.
Fig. 6 is that the ultrathin boron nitride nanosheet of this present example preparation carries out CO under full spectrum2+H2What O reacted
CO(a)、H2(b) and CH4(c) yield schematic diagram as can be seen from the figure compares the boron nitride of business, the hexagonal phase nitrogen of synthesis
Change boron nanometer sheet to CO2Conversion have good catalytic activity, and product is based on CO.
Fig. 7 is that the ultrathin boron nitride nanosheet of present example preparation is dispersed in water the schematic diagram to form colloid, can be with
Find out that the hexagonal phase boron nitride nanosheet of synthesis can be dispersed in water, the colloid of formation has Tyndall effect.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (8)
1. a kind of preparation method of ultrathin boron nitride nanosheet, which comprises the following steps:
(1) boric acid and urea are mixed in certain proportion and is put into tube furnace；
(2) cooled to room temperature obtains ultrathin boron nitride nanosheet after high temperature sintering under protective atmosphere.
2. the preparation method of ultrathin boron nitride nanosheet according to claim 1, which is characterized in that described in step (1)
The mass ratio of the mixture boric acid and urea that include be 1:1~1:50.
3. the preparation method of ultrathin boron nitride nanosheet according to claim 1, which is characterized in that in step (2), institute
The protective atmosphere stated is nitrogen or argon gas.
4. the preparation method of ultrathin boron nitride nanosheet according to claim 1, which is characterized in that described in step (2)
Protective atmosphere be nitrogen or argon gas when, gas flow rate be 30~1200 milliliters/per minute.
5. the preparation method of ultrathin boron nitride nanosheet according to claim 1, which is characterized in that described in step (2)
Heating rate be 1~15 DEG C/min.
6. the preparation method of ultrathin boron nitride nanosheet according to claim 1, which is characterized in that described in step (2)
Temperature be 500~1000 DEG C.
7. the preparation method of ultrathin boron nitride nanosheet according to claim 1, which is characterized in that described in step (2)
Soaking time be 2~15h.
8. the preparation method of ultrathin boron nitride nanosheet according to claim 1, which is characterized in that the boron nitride nanometer
The size of piece has visible light-responded in 1-4nm.
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Cited By (4)
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| CN109622019A (en) * | 2019-02-20 | 2019-04-16 | 哈尔滨工程大学 | The nitride-based catalyst and its method for treating water of nitrate in a kind of high efficiency photocatalysis reductive water |
| CN109777230A (en) * | 2019-02-25 | 2019-05-21 | 牟富书 | A kind of light catalyzed coating and preparation method thereof |
| CN110760099A (en) * | 2019-10-30 | 2020-02-07 | 安徽大学 | Preparation method of graphene-boron nitride nanotube heat-conducting filler and oriented heat-conducting composite material |
| CN112919431A (en) * | 2021-02-07 | 2021-06-08 | 辽东学院 | High-yield and high-crystallinity hexagonal boron nitride nanosheet and preparation method thereof |
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| CN110760099A (en) * | 2019-10-30 | 2020-02-07 | 安徽大学 | Preparation method of graphene-boron nitride nanotube heat-conducting filler and oriented heat-conducting composite material |
| CN112919431A (en) * | 2021-02-07 | 2021-06-08 | 辽东学院 | High-yield and high-crystallinity hexagonal boron nitride nanosheet and preparation method thereof |
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Application publication date: 20181218 |